KR20030025606A - Method of refining and microcapsuling tea extract - Google Patents

Abstract

PURPOSE: A method for purifying a high purity Theae folium extract containing tea polyphenol from a crude Theae folium extract and encapsulating the same is provided. The product contains 98% or more of tea polyphenol, therefore it can be effectively used as health supplementary foods or food additives. CONSTITUTION: A crude Theae folium extract is dissolved in purified water, agitated with Na2S2O4, EDTA-2Na, activated carbon and Al2O3 and then filtered. Thereafter, the filtrate is washed with purified water, added with NaCl, extracted in ethyl acetate two times, agitated with Al2O3 and MgSO4 and filtered. And the filtrate is agitated with methylene chloride at 0 to 5deg.C for 1hr, washed with methylene chloride and then dried.

Description

Purification and microencapsulation method of tea extract {Method of refining and microcapsuling tea extract}

The present invention relates to a tea extract containing high-purity tee polyphenols obtained from even extracts, and more particularly, to a method of extracting, separating and purifying tee polyphenols and microencapsulating them.

Tea has been ingested by humans for about 4000 years ago and is now the second most used beverage in the world after water. The types of tea can be divided into green tea, oolong tea or black tea. The production of green tea reaches 2.5 million tons per year, and the reason why tea is used as a worldwide drink is because it contains antioxidants in the tea, which is excellent for anti-aging and other effects. The main ingredient is known as polyphenol (polyphenol; catechin or tannine). come.

The research on the separation and physiological activity of the tea polyphenol has been conducted very actively for about 20 years. In foreign countries, it has been used for about 2 ~ 3 years for health supplements, food additives and functional cosmetics. It is being used and the amount used is increasing every year. This is due to the fact that the physiological activity of tea polyphenols is widely applied.

In other words, it significantly reduces serum cholesterol and prevents hypertension and arteriosclerosis, promotes oral health such as removing bad breath, and promotes fat, thereby preventing aging and preventing free radicals from being changed into lipid peroxide. This production prevents the destruction of collagen and elastin, which are important elements of the skin, prevents skin aging, hepatic protection and renal function, platelet aggregation and blood pressure strengthening, immunity increase and persistence, antimutagenic and obesity prevention. Many studies on bioactivity have been reported for improvement of digestive function, oral hygiene and oral health and bad breath removal effect.

In particular, a technology for separating tea polyphenols from green tea has been developed about two years ago, and localization has been successful in Korea. However, according to the conventional separation and purification method, the content of thiopolyphenol is very low, and the color of the product is dark brown, which makes it difficult to use as a health supplement, food additive or cosmetic.

The present invention has been made to solve the above problems, an object of the present invention is to provide a method for purifying tea extracts containing high-purity tea polyphenols from crude green tea extract and microencapsulates the food additives or health It can be used as a supplement.

An object of the present invention as described above, step (1) to make a solution by dissolving purified water in a ratio of 750 ml in 100 g of natural edodes extract; 15 g of Na ₂ S ₂ O ₄ , 5 g of EDTA-2Na, 20 g of activated carbon, and 16.7 g of Al ₂ O ₃ were added to the solution, followed by filtering after stirring; Adding (3) to the remaining filtrate after filtration, adding purified water at a rate of 100 ml, and adding and dissolving NaCl at a rate of 2 g to the filtrate (3);

Ethyl acetate (ethyl acetate) is added to the solution at a rate of 500 ml for primary extraction (4); Adding (5) ethyl acetate to the aqueous layer at a rate of 500 ml for secondary extraction; Adding 66.7 g of Al ₂ O ₃ and 60 g of MgSO ₄ to the extracted organic layer, followed by stirring and filtering (6);

Adding (7) the filtrate to another vessel filled with methylene chloride at a rate of 2 liters; Filtering after stirring at 0-5 ° C. for 1 hour (8); Washing (9) adding methylene chloride to the filtrate at a rate of 200 ml; And drying the filtrate to obtain a tea extract (10). A method of purifying tea extract, characterized in that consisting of.

The present invention provides a technique for mass-producing a product having a higher purity and whitening than a conventional product by extracting, separating, purifying and microencapsulating a tea extract containing high purity tea polyphenol from a low purity tea extract. Applied.

In addition, in the present invention, the tea extract containing the light yellow high purity thi polyphenol may be obtained by spray drying the ethyl acetate layer, which is an extraction solvent layer, in the middle of the purification process.

In addition, the present invention is characterized in that the above-mentioned tea extract is dissolved in ethanol or water and dried by spray drying to crystallize.

In the present invention, in order to obtain a micro-encapsulated product of tea extract containing high-purity tee polyphenol, the ethyl acetate layer extracted in the middle of refining is re-extracted with purified water to give carbohydrate, lactose, gelatin, dextine, amino acid or chitosan. It is encapsulated by crystallization by spray drying to obtain a variety of microcapsules of high purity green tea extract.

In the present invention, while improving the content of thiopolyphenol to 98% or more by using a chemical tablet purification method, the color of the product also improved the dark brown crude extract to the white color, the best color in the world.

Ethyl acetate, butanol, pentanol, etc. are used as the extraction solvent used in the present invention, methylene chloride, chloroform, n-hexane, etc. are used as the crystalline solvent, and activated carbon, Na ₂ S ₂ O ₄ , Na _It is characterized by using ₂ S ₂ O ₅ , Na ₂ SO ₃ , EDTA, Al ₂ O ₃ and the like. In addition, a variety of products can be prepared by microencapsulating various types of amino acids, carbohydrates, gelatin, lactose, dextine or chitosan for use in various food additives.

Other objects, specific advantages, and novel features of the present invention will become more apparent from the following detailed description of the invention and the preferred embodiments in connection with the accompanying drawings.

1 is a flowchart illustrating a method for purifying tea extract according to an embodiment of the present invention.

Hereinafter, a method for purifying and microencapsulating tea extract according to the present invention will be described in detail with reference to Examples.

<Example 1>

1 is a flowchart illustrating a method for purifying tea extract according to an embodiment of the present invention. As shown in FIG. 1, the first step is to prepare a solution by dissolving 100 g of natural even ethanol extract (tea polyphenol purity: 95.0%, dark brown) in 750 ml of purified water. In step ₂ , 15 g of Na ₂ S ₂ O ₄ , ₅ g of EDTA-2Na, 20 g of activated carbon, and 16.7 g of Al ₂ O ₃ were added to the solution, followed by stirring for 1 hour, followed by filtration.

The third step is to wash the remaining filtrate after filtration with 100 ml of purified water and dissolve by adding 20 g of NaCl to the filtrate. Step 4 is a step of first extraction with 500 mL of ethyl acetate in the solution. In the fifth step, 500 ml of ethyl acetate is added to the aqueous layer and the second extraction is performed. Step 6 is adding 16.7 g of Al ₂ O ₃ and 60 g of MgSO ₄ to the extracted organic layer, followed by stirring for 30 minutes and then filtering.

Subsequently, step 7 is a step of dropwise adding the filtrate to another container filled with 2 liters of methylene chloride for 1 hour. Step 8 is a step of filtering after stirring for 1 hour at 0 ~ 5 ℃. Step 9 is washing the filtrate with 200 ml of methylene chloride. Step 10 is to dry the filtrate to obtain a tea extract.

In this example, 92.0 g of an off-white target product was obtained. Caffeine (1.0% or less), epigallocatechin gallate (50% or more), gallocatechin gallate (16% or more), epicatechin gallate (epicatechin gallate) More than 22%.

<Example 2>

Even 100 g of extract (tea polyphenol 90.0%, dark brown) was purified as in Example 1 to obtain 80.3 g of the target and the purity and color were similar to Example 1.

<Example 3>

Even 100 g extract (tea polyphenol purity 80.0%, dark brown) was purified as in Example 1 to obtain the target product 71.2g and the purity and color was similar to Example 1.

<Example 4>

Even 100 g of extract (tea polyphenol purity 70.0%, dark brown) was purified as in Example 1 to obtain 62.8 g of the target and the purity and color were similar to Example 1.

Example 5

As shown in FIG. 1, step 30 after step 4 is to crystallize the ethyl acetate layer, which is an extraction solvent layer, by spray drying. The yield and analysis results of the target product in Example 5 were similar to the results of Examples 1 to 4.

<Example 6>

In the process of purifying in the same manner as in Examples 1 to 4, as shown in FIG. 1, step 40 after step 10 is a step of dissolving the tea extract in ethanol or water. Step 41 is a step of drying and crystallizing it by spray drying. Yield and analysis of the target product in Example 6 were similar to the results of Examples 1 to 4.

<Example 7>

In the process of purifying in the same manner as in Examples 1 to 4, as shown in FIG. 1, step 20 after step 5 is a step of primary extraction by adding water to the ethyl acetate layer at a rate of 700 ml. In step 21, water is added to the ethyl acetate layer at a rate of 300 ml to perform second extraction. Step 22 is to concentrate the extracted solution to about 1/2. Step 23 is a step of microencapsulating the concentrate by spray drying using carbohydrate, flavor, gelatin, lactose, dexine, amino acid or chitosan.

Here, the spray drying method is a method of adding excipients, emulsifiers, stabilizers, etc. to a core material, dissolving or suspending it in a solvent and spraying it with a nozzle or a disk, and at the same time instantaneously drying by inflow of hot air. Hot air is generally 150 ~ 200 ℃ high temperature, but because of the instantaneous removal of latent heat by the mechanical device can be encapsulated even relatively unstable heat. As the solvent evaporates rapidly, the coating becomes quite firm.

Table 1 below shows the results in Examples 1 to 4 comprehensively.

Crude Tea Polyphenols Yield Example 1 100 g (purity 95.0%, dark brown) 92.0 g (white) Example 2 100 g (purity 90.0%, dark brown) 80.3 g (white) Example 3 100 g (purity 80.0%, dark brown) 71.2 g (white) Example 4 100 g (purity 70.0%, dark brown) 62.8 g (white)

Purity of the targets obtained in Examples 1 to 7 were all 98% or more purity of polypolyphenol, 80% or more of catechin, 1.0% or less of caffein, 50% of epigallocatechin gallate. In the above, gallocatechin gallate (gallocatechin gallate) was more than 16%, epicatechin gallate (epicatechin gallate) was more than 22%. In addition, the purification was performed in the same manner for the natural tee polyphenol having a purity of 70% or less to obtain a white-white high purity product as in Examples 1 to 4 above.

The main physiological activity of the thiopolyphenol according to the present invention is a powerful antioxidant effect on free radicals or free radicals, which are harmful substances in the body, and anticancer by blocking the activity of urokinase that grows cancer cells. In addition to the foregoing, thi polyphenols increase the prevention of infectious diseases and increase the antibacterial ability by inhibiting the bacterial growth of the representative pathogenic bacteria, dysentery, typhoid, staphylococci and vibrio.

As mentioned above, according to the method for purifying the tea extract according to the present invention, it is possible to produce a product having a very high purity of polypolyphenol of 98% or more, and also to extract the dark brown crude extract to a white color. It can be easily used as a supplement for health supplements, food additives or cosmetics.

In addition, by using the micro-encapsulation of the tea polyphenol has a feature that can be widely used as a health supplement food or food additives of various fields by removing the bitter taste.

Although the present invention has been described in connection with the above-mentioned preferred embodiments, it is possible to make various modifications or variations without departing from the spirit and scope of the invention. Accordingly, the appended claims include such modifications and variations as fall within the spirit of the invention.

Claims (4)

Dissolving the natural edodes in purified water to form a solution (1); Na ₂ S ₂ O ₄ , EDTA-2Na, activated carbon, and Al ₂ O ₃ was added to the solution, followed by stirring and filtering (2); Washing with purified water the remaining filtrate after filtration and dissolving by adding NaCl to the filtrate (3); First extraction by adding ethyl acetate to the solution (4); Performing secondary extraction by adding ethyl acetate to the aqueous layer (5); Adding Al ₂ O ₃ and MgSO ₄ to the extracted organic layer, followed by stirring and filtering (6); Adding (7) the filtrate to another vessel filled with methylene chloride; Filtering after stirring at 0-5 ° C. for 1 hour (8); Washing by adding methylene chloride to the filtrate (9); And Drying the filtrate to obtain a tea extract (10); Purifying tea extract, characterized in that consisting of. The method according to claim 1, wherein the ethyl extract layer, which is the solvent layer of the extraction, is crystallized by spray drying. The method of claim 1, wherein the tea extract is dissolved in ethanol or water (40); And crystallizing by drying with a spray drying method (41). Primary extraction (20) by adding water to the ethyl acetate layer, which is the solvent layer for extraction according to claim 1; Performing secondary extraction by adding water to the ethyl acetate layer (21); Concentrating the extracted solution (22); And Microcapsule tea extract, characterized in that consisting of; microcapsule by spray drying method using carbohydrate, flavoring, gelatin, lactose, dextine, amino acid or chitosan for the concentrate (23).